Department of Pharmacology and Systems Physiology, College of Medicine, University of Cincinnati, 231 Albert Sabin Way, Cincinnati, OH 45267-0575, United States of America.
Department of Pharmacology and Systems Physiology, College of Medicine, University of Cincinnati, 231 Albert Sabin Way, Cincinnati, OH 45267-0575, United States of America.
J Immunol Methods. 2021 Sep;496:113103. doi: 10.1016/j.jim.2021.113103. Epub 2021 Jul 21.
In this work, we establish that cocaine binding to the Fab fragment of a recombinant humanized anti-cocaine mAb (h2E2) can be directly and easily quantitated using simple and inexpensive absorption and fluorescence measurements, employing dyes typically used for differential scanning fluorimetry, DASPMI and SYPRO Orange. For concentrated samples of the Fab fragment, absorbance spectroscopy employing these dyes reveals the number of cocaine sites present, using either DASPMI (by measuring the increase in dye absorbance) or SYPRO Orange (by measuring the change in dye maximal absorbance wavelength). Interestingly, we observed that cocaine binding to the Fab fragment had a much different effect on the SYPRO Orange dye absorbance than previously reported for the intact h2E2 mAb, resulting in a large decrease in the total dye absorbance for the Fab fragment, in contrast to previous results with the intact h2E2 mAb. For dilute samples of Fab fragment, a dye fluorescence emission spectroscopy assay was developed to quantitate the number of cocaine (and other high affinity cocaine metabolites) binding sites via the ligand-induced decrease in fluorescence emission of both of these extrinsic dyes. The difference in the cocaine titrations for the high affinity (Kd < 30 nM) ligands, cocaine, cocaethylene and benzoylecgonine and the low affinity (Kd > 30 μM) ligands, norcocaine, ecgonine methyl ester, and ecgonine were obvious using this assay. These simple, direct, and inexpensive techniques should prove useful for evaluation of other small molecule antigen binding Fab fragments, enabling quantitation and rapid biochemical assessments necessary for determining Fab fragment suitability for in vivo uses and other assays and experiments.
在这项工作中,我们确立了使用简单且廉价的吸收和荧光测量法,结合通常用于差示扫描荧光法(DASPMI)和 SYPRO Orange 的染料,可以直接且轻松地定量测定可卡因与重组人源化抗可卡因单克隆抗体(h2E2)Fab 片段的结合。对于 Fab 片段的浓缩样品,采用这些染料的吸收光谱法可以通过 DASPMI(通过测量染料吸光度的增加)或 SYPRO Orange(通过测量染料最大吸收波长的变化)来揭示存在的可卡因结合位点数量。有趣的是,我们观察到可卡因与 Fab 片段的结合对 SYPRO Orange 染料吸光度的影响与完整 h2E2 mAb 先前报道的有很大不同,导致 Fab 片段的总染料吸光度大幅下降,与先前用完整 h2E2 mAb 的结果相反。对于 Fab 片段的稀释样品,开发了一种染料荧光发射光谱测定法,通过这两种外源性染料的荧光发射的配体诱导降低来定量测定可卡因(和其他高亲和力可卡因代谢物)结合位点的数量。该测定法明显区分了高亲和力(Kd < 30 nM)配体,如可卡因、古柯烯和苯甲酰古柯碱,以及低亲和力(Kd > 30 μM)配体,如去甲可卡因、ecgonine 甲酯和 ecgonine 的可卡因滴定。这些简单、直接且廉价的技术应该对评估其他小分子抗原结合 Fab 片段有用,能够定量并快速进行生化评估,这对于确定 Fab 片段是否适合体内使用以及其他测定和实验是必要的。